普卢利沙星关键中间体的合成研究

Study on Synthesis of the Key Intermediate of Prulifloxacin

用螯合法把化合物6,7-二氟-1-甲基-4-氧代-4H-[1,3]噻嗪并[3,2-a]喹啉-3-羧酸乙酯与三乙酰氧化硼在DMSO中螯合,制得普卢利沙星的关键中间体6,7-二氟-1-甲基-4-氧代-4H-[1,3]噻嗪并[3,2-a]喹啉-3-羧基-O6,O7-二乙酸合硼,考察了不同溶剂、反应温度、反应时间对6,7-二氟-1-甲基-4-氧代-4H-[1,3]噻嗪并[3,2-a]喹啉-3-羧基-O6,O7-二乙酸合硼收率的影响。结果表明,所得产物的质量分数可达99.8%（HPLC归一法）,产率97.1%,质量分数和产率都比文献报道的高。

A novel synthetic route of 5,6-difluoro-1-methyl（-4-oxo-4H-thiazeto-quinoline-3-carboxylic-O6,O7-boron diethyl carboxylate（Ⅰ） was designed.The synthesis of（Ⅰ） from 5,6-difluoro-1-methyl（-4-oxo-4H-thiazeto-quinoline-3-carboxylic acid ethyl ester was performed by means of the Borlc coordination complex in this paper.The target compound was obtained by the Chelated Method.The reaction yield in different solvents,at different reaction temperatures and time were discussed in this paper.DMSO was finally used.The neutral titration was considered to be the best method in the hydrolysis reaction of the condensation product. The total yield was 97. 1%.